STRUCTURAL ELUCIDATION OF SOME NEW TITANACYCLES BY MEANS OF DEGRADATION AND 13C NMR STUDIES

Article abstract of DOI:10.1016/S0022-328X(00)82951-4

A reaction between diphenyltitanocene and phenyl(pentafluorophenyl)acetylene in refluxing benzene produces 1,1-bis(η⁵-cyclopentadienyl)-2-phenyl-3-(pentafluorophenyl)benzotitanole in 44percent yield.Degradation of the product with HCl/CHCl3 affords titanocene dichloride and Z-1,2-diphenyl-1-(pentafluorophenyl)ethene.Reaction of diphenyltitanocene and phenyl(pentafluorophenyl)acetylene in benzene under photolytic conditions results in the exclusive formation of 1,1-bis(η⁵-cyclopentadienyl)-2,5-diphenyl-3,4-di(pentafluorophenyl)titanole.The latter product can also be obtained in 77percent yield from a reaction between titanocene dicarbonyl and phenyl(pentafluorophenyl)acetylene in hexane solution.Application of 13C NMR spectroscopy to the structural elucidation of these and related metallacycles is discussed.